SABRE hyperpolarization enables high-sensitivity 1H and 13C benchtop NMR spectroscopy

Peter M. Richardson, Andrew J. Parrott, Olga Semenova, Alison Nordon, Simon B. Duckett, Meghan E. Halse

Research output: Contribution to journalArticle

11 Citations (Scopus)

Abstract

Benchtop NMR spectrometers operating with low magnetic fields of 1 – 2 T at sub-ppm resolution show great promise as analytical platforms that can be used outside the traditional laboratory environment for industrial process monitoring. One current limitation that reduces the uptake of benchtop NMR is associated with the detection fields reduced sensitivity. Here we demonstrate how para-hydrogen (p-H2) based signal amplification by reversible exchange (SABRE), a simple to achieve hyperpolarization technique, enhances agent detectability within the environment of a benchtop (1 T) NMR spectrometer so that informative 1H and 13C NMR spectra can be readily recorded for low-concentration analytes. SABRE-derived 1H NMR signal enhancements of up to 17,000-fold, corresponding to 1H polarization levels of P = 5.9%, were achieved for 52 mM pyridine in d4-methanol in a matter of seconds. Comparable enhancement levels can be achieved in both deuterated and protio solvents but now the SABRE-enhanced analyte signals dominate due to the comparatively weak thermally-polarized solvent response. The SABRE approach also enables the acquisition of 13C NMR spectra of analytes at natural isotopic abundance in a single scan as evidenced by hyperpolarized 13C NMR spectra of tens of millimolar concentrations of 4-methylpyridine. Now the associated signal enhancement factors are up to 45,500 fold (P = 4.0 %) and achieved in just 15 s. Integration of an automated SABRE polarization system with the benchtop NMR spectrometer framework produces renewable reproducible NMR signal enhancements that can be exploited for the collection of multi-dimensional NMR spectra, exemplified here by a SABRE-enhanced 2D COSY NMR spectrum.
LanguageEnglish
Pages3442-3450
Number of pages9
JournalAnalyst
Volume143
Issue number14
Early online date19 Jun 2018
DOIs
Publication statusPublished - 21 Jul 2018

Fingerprint

Nuclear magnetic resonance spectroscopy
Amplification
nuclear magnetic resonance
amplification
Magnetic Resonance Spectroscopy
spectroscopy
Nuclear magnetic resonance
Magnetic Fields
Methanol
Hydrogen
Spectrometers
spectrometer
Carbon-13 Magnetic Resonance Spectroscopy
polarization
Polarization
fold
Process monitoring
Proton Magnetic Resonance Spectroscopy
Pyridine
methanol

Keywords

  • benchtop NMR spectrometers
  • low magnetic fields
  • signal amplification by reversible exchange (SABRE)

Cite this

Richardson, Peter M. ; Parrott, Andrew J. ; Semenova, Olga ; Nordon, Alison ; Duckett, Simon B. ; Halse, Meghan E. / SABRE hyperpolarization enables high-sensitivity 1H and 13C benchtop NMR spectroscopy. In: Analyst. 2018 ; Vol. 143, No. 14. pp. 3442-3450.
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SABRE hyperpolarization enables high-sensitivity 1H and 13C benchtop NMR spectroscopy. / Richardson, Peter M.; Parrott, Andrew J.; Semenova, Olga; Nordon, Alison; Duckett, Simon B.; Halse, Meghan E.

In: Analyst, Vol. 143, No. 14, 21.07.2018, p. 3442-3450.

Research output: Contribution to journalArticle

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AU - Parrott, Andrew J.

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AU - Halse, Meghan E.

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